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| United States Patent |
5,585,092
|
|
Trandai
, et al.
|
December 17, 1996
|
Gel deodorant compositions
Abstract
The present invention relates to a gel deodorant composition comprising:
(a) from about 0.001% to about 50%, by weight of the composition, of
deodorant active, fragrance, or combination thereof; (b) from about 0.01%
to about 15%, by weight of the composition, of a soap gelling agent
selected from the group consisting of salts of C.sub.12 -C.sub.40 fatty
acids, and combinations thereof; (c) from about 3% to about 50%, by weight
of the composition, of glycerol, a polymer of glycerol, wherein said
polymer has a weight average molecular weight of about 800 or less, or
combinations thereof; (d) from about 5% to about 70%, by weight of the
composition, of one or more low molecular weight polyoxyethylene compounds
having a structure according to Formula (I):
##STR1##
wherein n is the interger 2, 3, 4, 5, 6, 7, or 8; R and R.sup.1 are,
independently, hydrogen; alkyl; or--C(.dbd.O)R.sup.2, where R.sup.2 is
hydrogen or alkyl; and (e) from about 8% to about 75%, by weight of the
composition, of water; wherein said composition contains no more than
about 15% propylene glycol, by weight of the composition.
| Inventors:
|
Trandai; Angie (West Chester, OH);
Jevtitch; Milan M. (Cincinnati, OH);
Phan; Dean V. (West Chester, OH);
Warner; Paulette L. (Cincinnati, OH)
|
| Assignee:
|
The Procter & Gamble Company (Cincinnati, OH)
|
| Appl. No.:
|
421644 |
| Filed:
|
April 13, 1995 |
| Current U.S. Class: |
424/65; 424/78.02; 424/78.08; 424/78.18; 424/401; 424/407; 512/1; 514/944; 514/946 |
| Intern'l Class: |
A61K 007/32 |
| Field of Search: |
424/65,400,401,407,78.02,78.08,78.18
512/1
514/944,946
|
References Cited
U.S. Patent Documents
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|
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|
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|
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|
| 4264586 | Apr., 1981 | Callingham et al. | 424/68.
|
| 4278655 | Jul., 1981 | Elmi | 424/47.
|
| 4278658 | Jul., 1981 | Hooper et al. | 424/65.
|
| 4280994 | Jul., 1981 | Turney | 424/68.
|
| 4338294 | Jul., 1982 | Mast | 424/68.
|
| 4346079 | Aug., 1982 | Roehl | 424/65.
|
| 4369173 | Jan., 1983 | Causland et al. | 424/35.
|
| 4511554 | Apr., 1985 | Geria et al. | 424/65.
|
| 4678663 | Jul., 1987 | Scott et al. | 424/62.
|
| 4695452 | Sep., 1987 | Gannis et al. | 424/59.
|
| 4708863 | Nov., 1987 | Bews et al. | 424/47.
|
| 4774079 | Sep., 1988 | Shin et al. | 424/66.
|
| 4814165 | Mar., 1989 | Berg et al. | 424/63.
|
| 4870010 | Sep., 1989 | Hayes | 424/114.
|
| 4921694 | May., 1990 | Hoppe et al. | 424/65.
|
| 5013473 | May., 1991 | Norbury et al. | 252/174.
|
| 5120541 | Jun., 1992 | Macaulay et al. | 424/401.
|
| 5128123 | Jul., 1992 | Brewster et al. | 424/65.
|
| 5162378 | Nov., 1992 | Guthauser | 514/785.
|
| 5194249 | Mar., 1993 | Drucker et al. | 424/68.
|
| 5198218 | Mar., 1993 | Kuznitz et al. | 424/401.
|
| 5221529 | Jun., 1993 | Tansley | 424/65.
|
| 5252711 | Oct., 1993 | Rogers et al. | 530/388.
|
| 5258174 | Nov., 1993 | Schebece | 424/65.
|
| 5271930 | Dec., 1993 | Walele et al. | 424/78.
|
| 5286755 | Feb., 1994 | Kauffmann et al. | 514/944.
|
| 5292503 | Mar., 1994 | Raleigh et al. | 424/59.
|
| 5316761 | May., 1994 | Brazinsky | 424/65.
|
| 5338541 | Aug., 1994 | Matz et al. | 424/71.
|
| 5364625 | Nov., 1994 | Sebag et al. | 424/401.
|
| 5374614 | Dec., 1994 | Behan et al. | 512/3.
|
| 5378468 | Jan., 1995 | Suffis et al. | 424/401.
|
| 5385729 | Jan., 1995 | Prencipe et al. | 424/70.
|
Primary Examiner: Mosley; Terressa
Attorney, Agent or Firm: Roof; Carl J., Winter; William J., Dabbiere; David K.
Claims
What is claimed is:
1. A gel deodorant composition comprising:
(a) from about 0.001% to about 50%, by weight of the composition, of
deodorant active, fragrance, or combination thereof;
(b) from about 0.01% to about 15%, by weight of the composition, of a soap
gelling agent selected from the group consisting of salts of C.sub.12
-C.sub.40 fatty acids, and combinations thereof;
(c) from about 3% to about 50%, by weight of the composition, of glycerol,
a polymer of glycerol, wherein said polymer has a weight average molecular
weight of about 800 or less, or combinations thereof;
(d) from about 5% to about 70%, by weight of the composition, of one or
more low molecular weight polyoxyethylene compounds having a structure
according to Formula (I):
##STR5##
wherein n is the interger 2, 3, 4, 5, 6, 7, or 8; R and R.sup.1 are,
independently, hydrogen; alkyl; or --C(.dbd.O)R.sup.2, where R.sup.2 is
hydrogen or alkyl; and
(e) from about 8% to about 75%, by weight of the composition, of water;
wherein said composition contains no more than about 15% propylene glycol,
by weight of the composition.
2. The gel deodorant composition of claim 1, wherein the soap gelling agent
is the salt of a fatty acid having from 14 to 20 carbon atoms.
3. The gel deodorant composition of claim 2, wherein the soap gelling agent
is selected from the group consisting of sodium stearate, sodium
palmitate, potassium stearate, potassium palmitate, and sodium myristate.
4. The gel deodorant composition of claim 2, wherein the soap gelling agent
is present in an amount from about 3% to about 7%.
5. The deodorant gel composition of claim 1, wherein the glycerol component
is present in an amount from about 8% to about 35%.
6. The gel deodorant composition of claim 5, wherein the glycerol component
is of the formula HOCH.sub.2 --CH(OH)--CH.sub.2 OH.
7. The gel deodorant composition of claim 6, wherein the polyoxyethylene
compound is present in an amount from about 10% to about 50%.
8. The gel deodorant composition of claim 7, wherein the polyoxyethylene
compound is present in an amount from about 15% to about 30%.
9. The gel deodorant composition of claim 7, wherein n is 2, 3, 4, or6.
10. The gel deodorant composition of claim 9, wherein n is 4.
11. The gel deodorant composition of claim 9, wherein R and R.sup.1 are
both hydrogen.
12. The gel deodorant composition of claim 1, wherein the weight ratio of
the glycerol component to the polyoxyethylene component is from about 1:5
to about 2: 1.
13. The gel deodorant composition of claim 12, wherein the weight ratio of
the glycerol component to the polyoxyethylene component is from about 1:3
to about 1: 1.
14. A gel deodorant composition comprising:
(a) from about 0.001% to about 10%, by weight of the composition, of
deodorant active, fragrance, or combination thereof;
(b) from about 1% to about 8%, by weight of the composition, of a soap
gelling agent selected from the group consisting of salts of C.sub.16
--C.sub.20 fatty acids, and combinations thereof;
(c) from about 8% to about 35%, by weight of the composition, of glycerol
having the structure HOCH.sub.2 --CH(OH)-13 CH.sub.2 OH or
2-hydroxypropylglyceryl ether;
(d) from about 15% to about 35%, by weight of the composition, of one or
more low molecular weight polyoxyethylene compounds having the structure
H(--OCH.sub.2 CH.sub.2 --).sub.n OH; where n is the integer 2, 3, 4, or 5;
and
(e) from about 15% to about 30%, by weight of the composition, of water;
wherein said composition contains no more than about 2% propylene glycol;
the weight ratio of the glycerol component to the polyoxyethylene
component is from about 1:1 to about 1:5; the combined weight of the
glycerol and polyoxyethylene components is from about 23% to about 45%;
and the gel deodorant is a gel stick having a penetration value of at
least about 60 tenths of a millimeter.
15. The gel deodorant composition of claim 14, wherein the deodorant active
is 2,4,4'-trichloro-2'hydroxy-diphenyl ether.
16. The gel deodorant composition of claim 15, wherein the soap gelling
agent is present in an amount of from about 3% to about 7%; with respect
to the polyoxyethylene component, n is 4; the weight ratio of the glycerol
component to the polyoxyethylene component is from about 1:1 to about 1:3;
and the gel stick has a penetration value of from about 70 to 160.
17. The gel deodorant composition of claim 16, wherein the soap gelling
agent is sodium stearate.
18. A method for controlling malodor comprising applying to the skin of a
human a safe and effective amount of the gel deodorant composition of
claim 1.
19. A method for controlling malodor comprising applying to the skin of a
human a safe and effective amount of the gel deodorant composition of
claim 14.
20. A method for controlling malodor comprising applying to the skin of a
human a safe and effective amount of the gel deodorant composition of
claim 17.
Description
FIELD OF INVENTION
This invention relates to gel deodorant compositions containing glycerol
and low molecular weight polyethylene glycol. These compositions provide
enhanced skin compatibility compared with known gel deodorant products.
BACKGROUND OF THE INVENTION Human body malodors are generally believed to
be caused in part by microbial interaction with sweat gland secretions
which produces pungent fatty acids. Aside from cleansing, one way such
odors are controlled is by the use of deodorant products, particularly in
the underarm area of the body.
Deodorant products generally contain a safe and effective level of perfume
or other odor masking ingredients, an antimicrobial active ingredient, or
a combination thereof, incorporated into a vehicle from which the active
ingredients may be deposited on the skin. Gel deodorant compositions have
several advantages over other types of stick formulations. For example,
they usually leave no more than a minimal amount of residue on the skin,
and they glide easily over the skin when applied. Deodorant compositions
of the gel type generally incorporate three key ingredients: a material
known to have deodorant efficacy, a gelling agent, and a polar solvent
system.
The gelling agents used most often in deodorant gel compositions are of the
fatty acid soap type. The gelling agents used in these compositions
include, for instance, the sodium or potassium salts of C.sub.12 -C.sub.22
fatty acids. These types of gel compositions most often utilize a highly
polar alcohol solvent as the primary polar solvent ingredient, which is
necessary to form the gel structure with the gelling agent. Monohydric and
dihydric alcohols, especially, propylene glycol and dipropylene glycol,
are typically used for this purpose.
Although alcohol/soap gel deodorants are quite popular and commonly used,
it is desirable to provide an improved deodorant gel composition that
exhibites improved mildness to the user. It is an object of the present
invention to provide such a composition. It is also an object of the
present invention to provide gel deodorant compositions having reduced
levels of polar solvents that can be relatively irritating to the skin,
e.g., mono- and dihydric alcohols such as propylene glycol and dipropylene
glycol, and to replace them with other ingredients. It is also an object
of the present invention to provide gel deodorant compositions having
minimal to essentially no propylene glycol. These and other benefits of
the present invention as may be disclosed or become apparent to those
skilled in the art can be obtained according to the invention described
below.
All percentages herein are by weight of the compositions unless otherwise
indicated, All ratios are weight ratios unless otherwise indicated.
All percentages, ratios, and levels of ingredients referred to herein are
based on the actual amount of the ingredient, and do not include solvents,
fillers, or other materials with which the ingredient may be combined as
commercially available products, unless otherwise indicated.
The invention hereof can comprise, consist of, or consist essentially of
the essential elements described herein as well as any of the preferred or
optional ingredients also described herein.
SUMMARY OF THE INVENTION
It has now been found that gel deodorant compositions with improved skin
compatibility can be obtained by incorporating into the soap-based product
both glycerol and low molecular weight polyethylene glycol as solvents.
The combination of these two mild solvent materials allows for
compositions which contain minimal to essentially no propylene glycol. The
combination also allows for reduction or elimination of dipropylene
glycol, a common solvent used in deodorant compositions that is not as
skin compatiable as the solvents used in the present invention. As a
result of this invention, gel deodorant compositions having improved skin
compatibility but still retaining overall gel rheology can be provided.
The compositions of the invention will contain no more than about 15%
propylene glycol. More preferably they will contain no more than about 10%
propylene glycol, still more preferably less than about 5%, most
preferably less than about 2%.
In addition to reducing to minimal levels, or eliminating, propylene glycol
and reducing the amount needed of other polyhydric alcohols, inclusion of
the glycerol and low molecular weight polyoxyethylene components provides
other benefits. Specifically, the glycerol component provides humectant
properties desirable in deodorant compositions. The polyoxyethylene
component eliminates the need to use excessively high levels of glycerol;
use of such high levels results in undesirable tackiness to many users.
Moreover, Applicants have discovered that low molecular weight
polyoxyethylene provides theological properties that allow smooth
application and efficient delivery of the gel deodorant.
Deodorant compositions comprising glycerol and polyoxyethylene are
described in co-pending application U.S. Ser. No. 08/307/951, filed Sep.
16, 1994, by Trandai and Phan. The compositions described in this
co-pending application also contain a polymeric gelling agent and a high
level of water. Applicants have discovered that the compositions of the
present invention, which do not contain such a gelling agent, are also
useful as deodorant gels.
In particular, this invention provides a gel deodorant composition
comprising:
(a) from about 0.001% to about 50%, by weight of the composition, of
deodorant active, fragrance, or combination thereof;
(b) from about 0.01% to about 15%, by weight of the composition, of a soap
gelling agent selected from the group consisting of salts of C.sub.12
-C.sub.40 fatty acids, and combinations thereof;
(c) from about 3% to about 50%, by weight of the composition, of glycerol
or a polymer of glycerol, wherein said polymer has a weight average
molecular weight of about 800 or less, or a combination thereof;
(d) from about 5% to about 70%, by weight of the composition, of one or
more low molecular weight polyoxyethylene compounds having a structure
according to Formula (I):
##STR2##
wherein n is the interger 2, 3, 4, 5, 6, 7, or 8; R and R.sup.1 are,
independently, hydrogen; alkyl; or --C(.dbd.O)R.sup.2, where R.sup.2 is
hydrogen or alkyl; and
(e) from about 8% to about 75%, by weight of the composition, of water;
wherein said composition contains no more than about 15%, by weight of the
composition, propylene glycol.
The deodorant products of the present invention relate to gel deodorant
compositions. These gel products may be in the form of solid sticks,
semi-solid sticks, or other softer, gel products. Most preferred is where
the gel products are in the form of a solid stick.
The present invention is described in more detail below.
DETAILED DESCRIPTION
The essential ingredients as well as a variety of preferred and optional
ingredients for the compositions of the present invention are described
below.
ESSENTIAL INGREDIENTS
Active Ingredients
The deodorant compositions hereof preferably comprise from about 0.001% to
about 50%, by weight, of a deodorant active, fragrance, or combination
thereof, preferably from about 0.01% to about 20%, more preferably from
about 0.1% to about 10%. Higher or lower levels are also contemplated and
intended to be encompasses as long as they are safe and effective for
topical application to the skin to control malodor. For purposes hereof, a
deodorant active shall be defined as an ingredient which prevents or
eliminates malodors from perspiration, as opposed to a fragrance which
covers or masks odors.
a. Deodorant Active Ingredients
Suitable types of deodorant actives include antimicrobial ingredients such
as bactericides and fungicides. Exemplary deodorant actives include
quaternary ammonium compounds such as cetyl-trimethylammonium bromide,
cetyl pyridinium chloride, benzethonium chloride, diisobutyl phenoxy
ethoxy ethyl dimethyl benzyl ammonium chloride, sodium N-lauryl sarcosine,
sodium N-palmethyl sarcosine, lauroyl sarcosine, N-myristoyl glycine,
potassium N-lauryl sarcosine, stearyl, trimethyl ammonium chloride, sodium
aluminum chlorohydroxy lactate, tricetylmethyl ammonium chloride,
2,4,4'-trichlorio-2'-hydroxy diphenyl ether, diaminoalkyl amides such as
L-lysine hexadecyl amide, heavy metal salts of citrate, salicylate, and
piroctose, especially zinc salts, and acids thereof, heavy metal salts of
pyrithione, especially zinc pyrithione and zinc phenolsulfate. Still other
antimicrobial ingredients include farnesol.
Other deodorant actives include odor absorbing materials such as carbonate
and bicarbonate salts, e.g. as the alkali metal carbonates and
bicarbonates, ammonium and tetraalkylammonium carbonates and bicarbonates,
especially the sodium and potassium salts.
Mixtures of deodorant actives are also contemplated and intended to be
encompassed herein.
b. Fragrance
The compositions of the present invention can contain a fragrance, or
perfume, to impart a desired aroma, or to mask odors that may be
associated with other components of the compositions. In the present
invention the fragrance is generally used at a level from about 0.01% to
about 10%.
Any fragrance suitable for application to the skin can be used herein
including a wide variety of fragrances and perfumes that are known to
those skilled in the art. The particular fragrance used is largely a
matter of choice; however, the fragrance should be used at a level
effective for providing a noticeable aroma to the composition, or for
masking undesired aroma of the composition. Also, the fragrance and
whatever carriers accompany it should not impart excessive stinging to the
skin, especially broken or irritated skin, at the levels previously
disclosed. The fragrance can be water soluble or water insoluble; however
it generally will be soluble in the composition hereof, typically in
either water or the polar solvent system.
Fragrances are made by those skilled in the art in a wide variety of
fragrances and strengths. Typical fragrances are described in Arctander,
Perfume and Flavour Chemicals (Aroma Chemicals), Vol. I and II (1969); and
Arctander, Perfume and Flavour Materials of Natural Origin (1960). U.S.
Pat. No. 4,322,308, Hooper et al., issued Mar. 30, 1982, and U.S. Pat. No.
4,304,679, Hooper et al., issued Dec. 8, 1981, both incorporated herein by
reference, disclose fragrance components as generally including, but are
not limited to, volatile phenolic substances (such as iso-amyl salicylate,
benzyl salicylate, and thyme oil red); essence oils (such as geranium oil,
patchouli oil, and petitgrain oil); citrus oils; extracts and resins (such
as benzoin siam resinoid and opoponax resinoid); "synthetic" oils (such as
Bergamot 37 and 430, Geranium 76 and Pomeransol 314); aldehydes and
ketones (such as B-methyl naphthyl ketone, p-t-butyl-A-methyl
hydrocinnamic aidehyde and p-t-amyl cyclohexanone); polycyclic compounds
(such as Coumarin and B-naphthyl methyl ether); esters (such as diethyl
phthalate, phenylethyl phenylacetate, non-anolide-1:4). Fragrances also
include esters and essential oils derived from floral materials and
fruits, citrus oils, absolutes, aldehydes, resinoides, musk and other
animal notes (e.g., natural isolates of civet, castoreum and musk),
balsamic, etc. and alcohols (such as dimyrcetol, phenylethyl alcohol and
tetrahydromuguol). Examples of such components useful in fragrances herein
include decyl aidehyde, undecyl aidehyde, undecylenic aidehyde, lauric
aidehyde, amyl cinnamic aidehyde, ethyl methyl phenyl glycidate, methyl
nonyl acetaldehyde, myristic aidehyde, nonalactone, nonyl aidehyde, octyl
aidehyde, undecalactone, hexyl cinnamic aidehyde, benzaldehyde, vanillin,
heliotropine, camphor para-hydroxy phenolbutanone, 6-acetyl 1,1,3,4,4,6
hexamethyl tetrahydronaphthalene, alpha-methyl ionone, gamma-methyl
ionone, and amyl-cyclohexanone and mixtures of these components.
Fragrance used in the present invention may also contain solubilizers,
diluents, or solvents which are well known in the art. Such materials are
described in Arctander, Perfume and Flavour Chemicals (Aroma Chemicals),
Vol. and II (1969). These materials typically include dipropylene glycol,
diethylene glycol, C.sub.1 -C.sub.6 alcohols, and benzyl alcohol.
Soap Gelling Agent
The compositions hereof will comprise from about 0.01% to about 15%, by
weight, of a soap gelling agent, preferably from about 0.1% to about 10%,
more preferably from about 1% to about 8%, most preferably from about 3%
to about 7%.
The soap gelling agents hereof are salts of fatty acids containing from
about 12 to about 40 carbon atoms (C.sub.12 -C.sub.40), preferably salts
of C.sub.12 -C.sub.22 fatty acids, more preferably C.sub.14 -C.sub.20,
most preferably C.sub.16 -C.sub.20. Suitable salt forming cations for use
in these gelling agents include metal salts such as alkali metals, e.g.
sodium and potassium, alkaline earth metals, e.g. magnesium, and aluminum.
Preferred are sodium and potassium salts.
Examples of fatty acids useful in synthesizing the gel forming agents
herein include myristic, palmitic, stearic, oleic, linoleic, linolenic,
margaric and mixtures of such acids. Naturally occurring sources of such
fatty acids include coconut oil, beef tallow, lanolin, fish oil, beeswax,
palm oil, peanut oil, olive oil, cottonseed oil, soybean oil, corn oil,
rapeseed oil, rosin acids, and greases.
Preferred fatty acid soap type gel forming agents include sodium stearate,
sodium palmitate, potassium stearate, potassium palmitate, sodium
myristate, and aluminum monostearate. The most preferred gel forming agent
is sodium stearate.
Mixtures of soap gelling agents can also be used.
Gycerol Component
The compositions of the present invention will comprise from about 3% to
about 50%, by weight, of glycerol or polyglycerol, preferably from about
6% to about 40%, more preferably from about 8% to about 35%, most
preferably from about 8% to about 20%.
The glycerol component is glycerol (i.e., HOCH.sub.2 CH(OH)CH.sub.2 OH); a
polymer of glycerol having a weight average molecular weight of about 800
or less; or mixtures thereof. Where a polyglycerol is used, preferred is
where the weight average molecular weight is about 500 or less, more
preferably 300 or less.
References herein to the glycerol component shall be understood to include
derivatives of glycerol. Suitable derivatives are alkyl ether derivatives
(preferably C.sub.1 -C.sub.18, more preferably C.sub.1 -C.sub.16, most
preferably C.sub.1 -C.sub.4). Exemplary alkyl ether derivatives include
ethyl, propyl, and butyl ether derivatives.
Also useful in the present compositions are the propoxylate glycerols
described in U.S. Pat. No. 4,976,953, issued Dec. 11, 1990 to Orr and
Sabatelli, which is incorporated by reference herein.
Most preferred are compositions that contain glycerol, per se, not glycerol
derivatives or polyglycerols.
Polyoxyethylene Component
The compositions of the present invention will comprise from about 5% to
about 70%, by weight, of a polyoxyethylene (hereafter "POE") component,
preferably from about 10% to about 50%, more preferably from about 15% to
about 35%, most preferably from about 15% to about 30%.
The polyoxyethylene compounds used herein are low molecular weight
polyethylene glycols (hereafter "PEGS"), or full or partial ethers or
esters thereof. These compounds have a structure according to the
following formula:
##STR3##
wherein R and R.sup.1 are, independently, hydrogen; alkyl; or
--C(.dbd.O)R.sup.2, wherein R.sup.2 is hydrogen or alkyl. When R is alkyl
or --C(.dbd.O)R.sup.2, both R and R.sup.1 are the same. This is where the
POE is a PEG-diether derivative or a PEG-diester derivative. When R is
hydrogen, R.sup.1 can be hydrogen (a PEG), alkyl (PEG-monoether), or
--C(.dbd.O)R.sup.2 (PEG-monoester).
Particularly preferred are compostions wherein both R and R.sup.1 are
hydrogen.
In this formula, n is an interger from 2 to 8, which relates to PEGs having
an average degree of ethoxylation of 2 to 8. Preferred is where n is from
2 to 6, more preferably 2 to 5, most preferably 4.
The total combined amount of glycerol and POE, by weight of the
composition, is from about 8% to about 70%. Where a higher level of this
combination is used, the compositions provide decreased performance, and
reduced end-user satisfaction. The total combined amount is preferably
from about 15% to about 50%, more preferably about 23% to about 45%, most
preferably from about 25% to about 40%.
The weight ratio of the glycerol component to the POE component is from
about 1:10 to about 5:1, preferably about 1:5 to about 2:1, more
preferably about 1:3 to about 1:1; most preferably from about 1:2 to about
1:1.
Other polar solvents may be used in the present compositions as optional
ingredients. These include, for example, monohydric C.sub.2 -C.sub.10
alkyl alcohols, dihydric C.sub.3 -C.sub.12 alkyl alcohols other than
propylene glycol, alkyl ethers thereof (preferably C.sub.1 -C.sub.4 alkyl
ethers), and mixtures thereof.
Examples of such optional solvents include dipropylene glycol, tripropylene
glycol, ethanol, n-propanol, n-butanol, t-butanol, 2-methoxyethanol,
2-ethyoxyethanol, ethylene glycol, isopropanol, isobutanol, 1,4-butylene
glycol, 1,2-butylene glycol, 1,3-butylene glycol, 2,3-butylene glycol,
2,4-dihydroxy-2-methylpentane; trimethylene glycol, 1,3-butane diol,
1,4-butane diol, and the like, and mixtures thereof.
Monohydric alcohols used herein not only provide solvency, but also provide
certain cosmetic advantages such as cool feel to the skin and a strong
scent which confirms the deodorant's presence to the user. Preferred
monohydric alcohols for such purpose include, for example, methanol,
ethanol, isopropanol, and mixtures thereof; most preferred is ethanol.
The level of mono- and di- hydric C.sub.1 -C.sub.12 alcohols, especially
the C.sub.1 -C.sub.6 alcohols, in the present compositions should
generally be no more than about 50%, by weight of the composition,
preferably no more than about 35%, more preferably no more than about 30%,
even more preferably no more than about 25%, and most preferably from 0%
to no more than about 15%.
Optional polar solvents useful in the present invention also include, for
example, propylene carbonate and 3-methyl-2-oxazolidinone.
Water
The compositions of the present invention will comprise from about 8% to
about 75%, by weight, water, preferably from about 10% to about 60%, more
preferably from about 15% to about 50%, most preferably from about 15% to
about 30%.
NON-ESSENTIAL INGREDIENTS
Hydrogel Forming Polymeric Gelling Agent
The deodorant compositions of the present invention may comprise aqueous
gel formed from a highly absorbent hydrogel forming polymeric gelling
agent. As discussed above, such compositions are described in co-pending
application U.S. Ser. No. 08/307,951. An advantage provided by inclusion
of a hydrogel forming polymeric gelling agent is that increased levels of
water can be included in the compositions.
The compositions may contain from about 0.001% to about 5%, by weight of
the composition, preferably from about 0.01% to about 5%, more preferably
from about 0.05% to about .1%, most preferably from about 0.1% to about
0.75% of such hydrogel forming polymeric gelling agent, calculated based
on the dry weight of the hydrogel forming polymeric gelling agent.
The optional hydrogel forming polymeric gelling agent hereof is highly
absorbent of water, and will generally be able to absorb at least about 40
g water (deionized) per gram of gelling agent, preferably at least about
60 g/g, more preferably at least about 80 g/g. These values, referred to
as "Absorptive Capacity" herein can be determined according to the
procedure in the Absorptive Capacity "Tea Bag" test in the Experimental
Section below.
The hydrogel forming polymeric gelling agent hereof will also preferably be
characterized by an extractable polymer content of (e) of no more than
about 20%, more preferably no more than about 12%, most preferably no more
than about 10%. The extractable polymer content (e) is determined
according to the procedures set forth in the Experimental Section, below.
The hydrogel forming polymeric material, when in dry form, will generally
be in the form of particles or fibers. Particles will preferably have a
weight average particle size (diameter, or equivalent diameter in the case
of non-spherical particles) of from about 5 to about 500 microns,
preferably from about 10 to about 60 microns, more preferably from about
10 to about 50 microns. Fibrous hydrogel forming polymeric gelling agent
preferably have diameters (or equivalent diameters in the case of
non-round fibers) of from about 5 to about 100 microns, preferably from
about 15 to about 50 microns, and lengths of from about 0.1 mm to about 5
mm more preferably from about 0.5 mm to about 2 mm. It is contemplated
that larger or smaller particles or fibers can be used, although they are
not preferred, as larger particles or fibers may provide a grainier or a
more string-like product feel, and smaller particles may result in
processing difficulties. If relatively large particles or fibers are used
during manufacture, improved finished product aesthetics can be obtained
by sheer mixing the compositions or other mixing operations during
processing of the compositions.
In general, the hydrogel forming polymeric gelling agent materials
optionally used in the present invention are at least partially
crosslinked polymers prepared from polymerizable, unsaturated
acid-containing monomers which are water-soluble or become water-soluble
upon hydrolysis. These include monoethylenically unsaturated compounds
having at least one hydrophilic radical, including olefinically
unsaturated acids and anhydrides which contain at least one carbon-carbon
olefinic double bond.
With respect to these monomers, water-soluble means that the monomer is
soluble in deionized water at 25.degree. C. at a level of at least 0.2%,
preferably at least 1.0%.
Upon polymerization, monomeric units as described above will constitute
from about 25 mole percent to 99.99 mole percent, more preferably from
about 50 mole percent to 99.99 mole percent, most preferably at least
about 75 mole percent of the polymeric gelling agent material (dry polymer
weight basis). Two or more different monomer types of the previously
described acid group-containing monomers may be copolymerized in order to
provide the hydrogel-forming polymeric gelling material. Exemplary types
of such acid groups and other hydrophilic groups include carboxyl,
carboxylic acid anhydride, carboxylic salt, sulfonic acid, sulfonic acid
salt, hydroxyl, ether, amide, amino and ammonium salt groups.
Hydrogel forming polymeric gelling agents suitable for use herein are well
known in the art, and are described, for example, in U.S. Pat. No.
4,076,663, Masuda et al., issued Feb. 28, 1978; U.S. Pat. No. 4,062,817,
Westerman, issued Dec. 13, 1977; U.S. Pat. No. 4,286,082, Tsubakimoto et
al., issued Aug. 25, 1981; U.S. Pat. No. 5,061,259, Goldman et al., issued
Oct. 29, 1991, and U.S. Pat. No. 4,654,039, Brandt et al., issued Mar. 31,
1987 all of which are incorporated herein in their entirety.
Hydrogel forming polymeric gelling agents suitable for use herein are also
described in U.S. Pat. No. 4,731,067, Le-Khac, issued Mar. 15, 1988, U.S.
Pat. No. 4,743,244, Le-Khac, issued May 10, 1988, U.S. Pat. No. 4,813,945,
Le-Khac, issued Mar. 21, 1989, U.S. Pat. No. 4,880,868, Le-Khac, issued
Nov. 14, 1989, U.S. Pat. No. 4,892,533, Le-Khac, issued Jan. 9, 1990, U.S.
Pat. No. 5,026,784, Le-Khac, issued Jun. 25, 1991, U.S. Pat. No.
5,079,306, Le-Khac, issued Jan. 7, 1992, U.S. Pat. No. 5,151,465, Le-Khac,
issued Sep. 29, 1992, U.S. Pat. No. 4,861,539, Allen, Farrer, and Flesher,
issued Aug. 29, 1989, and U.S. Pat. No. 4,962,172, Allen, Farrer, and
Flesher, issued Oct. 9, 1990, all incorporated herein by reference in
their entireties.
Examples of suitable water-soluble monomers from which monomer units of the
polymers hereof can be derived are as follows:
1. Carboxyl group-containing monomers (carboxylic acid-containing):
monoethylenically unsaturated mono or poly-carboxylic acids, such as
(meth) acrylic acid (meaning acrylic acid or methacrylic acid; similar
notations are used hereinafter), maleic acid, fumaric acid, sorbic acid,
itaconic acid, citraconic acid, tricarboxy ethylene, and ethacrylic acid;
2. Carboxylic acid anhydride group-containing monomers: monoethylenically
unsaturated polycarboxylic acid anhydrides, such as maleic anhydride;
3. Carboxylic acid salt-containing monomers: water-soluble salts 0 (alkali
metal salts, ammonium salts, amine salts, etc.) of monoethylenically
unsaturated mono- or poly- carboxylic acids [such as sodium
(meth)acrylate, trimethylamine (meth)acrylate, triethanolamine (meth)
acrylate, sodium maleate, methylamine maleate];
4. Sulfonic acid group-containing monomers: aliphatic or aromatic 5 vinyl
sulfonic acids (such as vinylsulfonic acid, allyl sulfonic acid,
vinyltoluenesulfonic acid, styrene sulfonic acid), (meth)acrylic sulfonic
acids [such as sulfopropyl (meth) acrylate, 2-hydroxy-3-(meth)acryloxy
propyl sulfonic acid, 2-acylamido-2-methyl propane sulfonic acid];
5. Sulfonic acid salt group-containing monomers: alkali metal salts,
ammonium salts, amine salts of sulfonic acid group-containing monomers as
mentioned above.
6. Hydroxyl group-containing monomers: monoethylenically unsaturated
alcohols [such as (meth)allyl alcohol], monoethylenically unsaturated
ethers or esters of polyols (alkylene glycols, glycerol, polyoxyalkylene
polyols), such as hydroxethyl (meth)acrylate, hydroxypropyl
(meth)acrylate, triethylene glycol (meth)acrylate, poly(oxyethylene
oxypropylene) glycol mono (meth)allyl ether (in which hydroxyl groups may
be etherified or esterified).
7. Amide group-containing monomers: (meth) acrylamide, N-alkyl
(meth)acrylamides (such as N-methylacrylamide, N-hexylacrylamide),
N,N-dialkyl (meth)acryl amides (such as N,N-dimethylacrylamide,
N,N'-di-n-propylacrylamide), N-hydroxyalkyl (meth)acrylamides [such as
N-methylol(meth)acrylamide, N-hydroxyethyl (meth)acrylamide],
N,N-dihydroxyalkyl (meth)acrylamides [such as N,N-dihydroxyethyl
(meth)acrylamide], vinyl lactams (such as N-vinylpyrrolidone);
8. Amino group-containing monomers: amino group-containing esters (e.g.
dialkylaminoalkyl esters, dihydroxyalkylaminoalkyl esters, morpholinoalkyl
esters, etc. ) of monoethylenically unsaturated mono- or dicarboxylic acid
[such as dimethlaminoethyl (meth)acrylate, diethylaminoethyl
(meth)acrylate, morpholinoethyl (meth)acrylate, dimethyl aminoethyl
fumarate], heterocyclic vinyl compounds [such as vinyl pyridines (e.g.
2-vinyl pyridine, 4-vinyl pyridine, N-vinyl pyridine), N-vinyl imidazol];
and
9. Quaternary ammonium salt group-containing monomers:
N,N,N-trialkyI-N-(meth)acryloyloxyalkylammonium salts [such as
N,N,N-trimethyl-N-(meth)acryloyloxyethylammonium chloride,
N,N,N-triethyl-N-(meth)acryloyloxyethylammonium chloride,
2-hydroxy-3-(meth)-acryloyloxypropyl trimethyl ammonium chloride], and
monomers as mentioned in British patent specification No. 1,034,296.
Suitable monomers which become water-soluble by hydrolysis, for use in this
invention instead of or in conjunction with the water-soluble 5 monomers,
include monethylenically unsaturated compounds having at least one
hydrolyzable group, such as ester and nitrile groups. Such monomers having
an ester group include for example, lower alkyl (C1-C3) esters of
monoethylenically unsaturated carboxylic acids, such as methyl
(meth)acrylate, ethyl (meth)acrylate and 2-ethylhexyl (meth)acrylate; and
esters of monoethylenically unsaturated alcohols [vinyl esters,
(meth)-allyl ester, etc.], such as vinyl acetate and (meth) allyl acetate.
Suitable nitrile group-containing monomers include (meth) acrylonitrile.
Preferred monomers include carboxylic acid monomers, or anhydrides or salts
thereof. Especially preferred monomers include acrylic acid, methacrylic
acid, and maleic acid, and anhydrides and salts thereof. Acrylic acid and
combinations of acrylic acid and acrylate salt (e.g. sodium acrylate) are
particularly preferred.
While at least 25 mole percent (preferably at least about 35%, more
preferably at least about 50%) of the hydrogel-forming polymer
compositions herein should be prepared-from acid group-containing
monomers, some non-acid monomers may also be used to prepare the
hydrogel-forming polymer compositions herein (prior to neutralization). It
is particularly useful to incorporate non-acid monomers into polymers to
be formed into fibers, in order to increase the flexibility of the final
polymeric material. Such non-acid monomers can include, for example, the
water-soluble or water-dispersible esters of the foregoing acid-containing
monomers as well as monomers which contain no carboxyl or sulfonic acid
groups at all. Optional non-acid monomers can thus include, for example,
carboxylic acid or sulfonic acid ester-containing monomers e.g. C.sub.1
-C.sub.4 esters, hydroxyl group-containing monomers, amide
group-containing monomers, amino group-containing monomers, nitrile group
containing monomers, quaternary ammonium salt group-containing monomers
and unsaturated polymerzable hydrocarbons, such as alph-olefins, vinyl
monomers, and vinylidene monomers. Examples include ethylene, propylene,
isobutylene, 1-butylene, vinyl acetate, methyl vinyl ether, isobutyl vinyl
ether, and styrene compounds of the formula:
##STR4##
wherein R represents H or a C.sub.1 -C.sub.6 alkyl, and wherein the
benzene ring may be substituted with low molecular weight alkyls (e.g.
C.sub.1 -C.sub.4) or hydroxy groups. These non-acid monomers are well
known materials and are 5 described in greater detail, for example, in
Masuda et al., U.S. Pat. No. 4,076,663, issued Feb. 28, 1978; and in
Westerman, U.S. Pat. No. 4,062,817, issued Dec. 13, 1977; and U.S. Pat.
No. 5,151,465 Le-Khac, issued Sep. 29, 1992; each of which are already
incorporated herein by reference. If present at all, such non-acid
monomers should generally be used only to such an extent that, prior to
neutralization, no more than 75% mole percent of the polymer compositions
herein are prepared from such non-acid monomers, preferably no more than
about 65%, more preferably no more than about 50%.
Especially preferred are copolymers of maleic acid, maleic anhydride, or
malic acid salt with isobutylene or other C.sub.3 -C.sub.6, preferably
C.sub.4, vinyl monomers most preferably isobutylene at a mole precent of
from about 35% to about 65% maleic monomer units to about 65% to about 35%
isobutylene or other C.sub.3 -C.sub.6 vinyl monomers.
In the hydrogel-forming polymeric gelling agent the polymeric component
formed from unsaturated, acid-containing monomers may be grafted on to
other types of polymer moleties such as starch or cellulose.
Suitable starches include, for example, natural starches such as sweet
potato starch, potato starch, wheat starch, corn starch, rice starch,
tapioca starch, and the like, and processed or modified starches such as
alpha-starch, dextrine, oxidized starch, dialdehyde starch,
alkyl-etherified starch, allyl-etherified starch, oxyalkylated starch,
aminoethyl-etherified starch, cyanoethyl-etherified starch and the like.
Suitable celluloses include, for example, celluloses obtained from wood,
leaves, stems, bast, seed fluffs, and the like; and modified celluloses
such as alkyl-etherified cellulose, organic-acid-esterified cellulose,
oxidized cellulose, hydrocellulose, and the like. Starch grafted materials
of this type are especially preferred for use herein.
Whatever the nature of the monomer components of the hydrogel-forming
polymeric gelling agents used in the present compositions, the polymers
thereof will be crosslinked. Suitable cross-linking agents are well know
in the art and include, for example, (1) compounds having at least two
polymerizable double bonds; (2) compounds having at least one
polymerizable double bond and at least one functional group reactive with
the acid-containing monomer material; (3) compounds having at least two
functional groups reactive with the acid-containing monomer material; and
(4) polyvalent metal compounds which can form ionic cross-linkages.
Cross-linking agents having at least two polymerizable double bonds include
(i) di- or polyvinyl compounds such as divinylbenzene and divinyltoluene;
(ii) di- or poly-esters of unsaturated mono- or poly-carboxylic acids with
polyols including, for example, di- or triacrylic acid esters of polyols
such as ethylene glycol, trimethylol propane, glycerine, or
polyoxyethylene glycols; (iii) bisacrylamides such as
N,N-methylenebisacrylamide; (iv) carbamyl esters that can be obtained by
reacting polyisocyanates with hydroxyl group-containing monomers; (v)
di-or poly-allyl ethers of polyols; (vi) di- or poly-allyl esters of
polycarboxylic acids such as diallyl phthalate, diallyl adipate, and the
like; (vii) esters of unsaturated mono- or poly-carboxylic acids with
mono-allyl esters of polyols such as acrylic acid ester of polyethylene
glycol monoallyl ether; and (viii) di- or tri-allyl amine.
Cross-linking agents having at least one polymerizable double bond and at
least one functional group reactive with the acid-containing monomer
material include N-methylol acrylamide, glycidyl acrylate, and the like.
Suitable cross-linking agents having at least two functional groups
reactive with the acid-containing monomer material include glyoxal;
polyols such as ethylene glycol and glycerol; polyamines such as alkylene
diamines (e.g., ethylene diamine ), polyalkylene polyamines, polyepoxides,
di- or polyglycidyl ethers and the like. Suitable polyvalent metal
cross-linking agents which can form ionic cross-linkages include oxides,
hydroxides and weak acid salts (e.g., carbonate, acetate and the like) of
alkaline earth metals (e.g., calcium, magnesium) and zinc, including, for
example, calcium oxide and zinc diacetate.
Cross-linking agents of many of the foregoing types are described in
greater detail in Masuda et al., U.S. Pat. No. 4,076,663, issued Feb. 28,
1978, and Allen et al., U.S. Pat. No. 4,861,539, issued Aug. 29, 1989,
both incorporated herein by reference. Preferred cross-linking agents
include the di- or polyesters of unsaturated mono- or polycarboxylic acids
mono-allyl allyl esters of polyols, the bisacrylamides, and the di- or
tri-allyl amines. Specific examples of expecially preferred cross-linking
agents include N,N'-methylenebisacrylamide and trimethylol propane
triacrylate.
The cross-linking agent will generally constitute from about 0.001 mole
percent to 5 mole percent of the resulting hydrogel-forming polymeric 5
material. More generally, the cross-linking agent will constitute from
about 0.01 mole percent to 3 mole percent of the hydrogel-forming
polymeric gelling agent used herein.
The hydrogel forming polymeric gelling agent herein is at least partially
crosslinked, however the degree of crosslinking must be high enough such
that the resulting polymer does not exhibit a glass transition temperature
(Tg) below about 140.degree. C., and accordingly, the term "hydrogel
forming polymeric gelling agent," as used herein, shall mean polymers
meeting this parameter. Preferably the hydrogel forming polymeric gelling
agent does not have a Tg below about 180.degree. C., and more preferably
does not have a Tg prior to decomposition of the polymer, at temperatures
of about 300.degree. C. or higher. The Tg can be determined by
differential scanning calorimetry (DSC) conducted at a cooling rate of
20.0 C..degree./minute with 5 mg or smaller samples. The Tg is calculated
as the midpoint between the onset and endset of heat flow change
corresponding to the glass transition on the DSC heat capacity cooling
curve. The use of DSC to determine Tg is well known in the art, and is
described by B. Cassel and M.P. DiVito in "Use of DSC To Obtain Accurate
Thermodynamic and Kinetic Data", American Laboratory, January 1994, pp
14-19, and by B. Wunderlich in Thermal Analysis, Academic Press, Inc.,
1990.
The hydrogel forming polymeric gelling agents hereof are preferably
employed in their partially neutralized form. For purposes of this
invention, such materials are considered partially neutralized when at
least 25 mole percent, and preferably at least 50 mole percent of monomers
used to form the polymer are acid group-containing monomers which have
been neutralized with a base. Suitable neutralizing bases cations include
hydroxides of alkali and alkaline earth metal (e.g. KOH, NaOH), ammonium,
substituted ammonium, and amines such as amino alcohols (e.g.,
2-amino-2-methyl-1,3-propanediol, diethanolamine, and
2-amino-2-methyl-1-propanol. This percentage of the total monomers
utilized which are neutralized acid group-containing monomers is referred
to herein as the "degree of neutralization". The degree of neutralization
will preferably not exceed 98%.
Hydrogel forming polymer gelling agent materials can be prepared by
reacting monomers and cross-linking agents, as described above, in
conventional manners. Prior art hydrogel forming polymeric gelling agent
synthesis procedures are well known in the art and are also disclosed, for
example, in the previously referenced U.S. Pat. Nos. 4,654,039, 4,286,082,
and 4,340, 706.
Suitable hydrogel forming polymeric gelling agents in the form of particles
are commercially available from Hoechst Celanese Corporation, Portsmouth,
VA, USA (Sanwet.TM. Superabsorbent Polymers) Nippon Shokubai, Japan
(Aqualic.TM., e.g., L-75, L-76) and Dow Chemical Company, Midland, MI, USA
(Dry Tech.TM.).
Suitable hydrogel forming polymeric gelling agents in the form of fibers
are commercially available from Camelot Technologies Inc., Leominster, MA,
USA (Fibersorb.TM., e.g., SA 7200H, SA 7200M, SA 7000L, SA 7000, and SA
7300).
Other Optional Ingredients
A wide variety of additional optional ingredients can be incorporated into
the present compositions. These include components for improving
cosmetics, efficacy, stability, and aesthetics. Such optional ingredients
include: emollients; humectants; soothing agents; dyes and pigments;
medicaments; pH buffering agents; fillers; and the like.
Buffering agents include coconut monoethanolamide, sodium hydroxide,
stearamide, monoethanolamide, acetamide MEA, zinc acetate, sodium
chloride, potassium chloride, zinc stearate, aluminum oxide, calcium
acetate, zinc oxide, magnesium oxide, calcium carbonate, calcium
hydroxide, sodium carbonate, magnesium carbonate, zinc carbonate, calcium
oxide, and mixtures thereof.
Fillers include silicate powders such as talc, aluminum silicate, magnesium
silicate, metallic stearates, polyethylene, colloidal silica, clays such
as bentonire, and particulate hydrophilic polymers such as cellulose ether
polymers, modified starches, polyamides, and polypeptides.
Soothing agents are ingredients that can mitigate irritation to the skin
caused by other ingredients or pre-existing conditions (e.g. burns,
stings, redness, rash, abrasions, cuts etc.). Exemplary soothing agents
include aloe vera, allantoin, D-panthenol, avocado oil and other
vegetative oils, and lichen extract.
COMPOSITIONS
The compositions can be provided in a variety of product rheologies,
including both soft and hard gels. However the preferred compositions will
be hard gels (sticks) having a Penetration Value of at least about 60
(measured in tenths of a millimeter), preferably from about 65-200, more
preferably from about 70 to about 160, most preferably from about 75 to
about 120. Penetration Value is determined according to the standard
procedure set forth by ASTM Method D-5 for gel stick compositions stored
prior to testing at about 26.7.degree. C. (80.degree. F.) for at least 24
hours, using an automatic fixed time penetrometer (e.g. Fisher Scientific
Co., Model 13-399-10 or equivalent) and a taper-tipped penetration needle
as specified in ASTM Method D 1321-DIN 51 579. The total weight of the
needle and shaft in the penetrometer is 50.00.+-.0.05 grams.
METHOD OF MANUFACTURE
The compositions of the present invention may be made by any of the typical
methods known in the art for formulating deodorant gel compositions. As
will be apparent to those skilled in the art, the particular method will
be dependent upon the selection of the specific types and amounts of the
components employed.
In general, the compositions of the present invention can be prepared by
mixing water, the glycol component, the polyoxyethylene component, the
deodorant active (if applicable), and preservative (if applicable). The
mixture is stirred and heated to a temparature from about 75-90.degree. C.
While stirring, the gelling agent is added. When the solution is clear, a
buffering agent may be added. The solution is cooled and a fragrance (if
applicable) is added. The composition is packaged in coventional deodorant
dispenser at about 70.degree. C., and cooled to room temperature.
Where a polymeric hydrogel forming material is included in the composition,
those skilled in the art will recognize that the particular method will be
dependent upon the selection of the polymeric hydrogel.
In general, the compositions can be made as follows: Prepare a premix A of
the hydrogel forming polymeric gelling agent and water and then mix to
form a homogenous gel. Optionally shear mix to reduce gel particle size
and improve smoothness to the touch. Prepare a premix B with the soap
gelling agent, and the polyhydroxy solvent for the soap gelling agent,
with mixing at a temperature high enough to dissolve the soap gelling 10
agent (typically about 70.degree.-95.degree. C.). Combine premixes A and B
with mixing and preferably cool to about 60.degree.-80.degree. C. if
additional volatile ingredients are to be added. Add other ingredients, as
may be applicable, to either premix or to the final mixture prior to
cooling below the set point of the soap gel. Mix and cool to below the set
point of the soap gel.
METHOD FOR USE
The present invention provides methods for controlling malodor. These
methods comprise applying to the skin of a human a safe and effective
amount of the gel deodorant composition of the present invention. The term
"a safe and effective amount" as used herein, is an amount which is
effective in eliminating or substantially reducing malodor associated with
human underarm perspiration while being safe for human use at a reasonable
risk/benefit ratio. Typically, the safe and effective amount used is from
about 0.1 gram per axilla to about 2.0 gram per axilla.
EXPERIMENTAL
The following experimental disclosure relates to gel deodorant compositions
comprising the optional hydrogel forming polymeric gelling material
discussed above.
a. Absorptive Capacity "Tea Bag" Test
Absorptive Capacity can be determined by a gravimetric analytical technique
using deionized water as the fluid for which Absorptive Capacity of the
polymeric gelling agent is to be calculated. A sample of polymeric gelling
agent is placed within a tea bag, immersed in an excess of deionized water
for a specified period of time, and then centrifuged for a specific period
of time. The ratio of polymeric gelling agent final weight after
centrifuging minus initial weight (net fluid gain) to initial weight
determines the Absorptive Capacity.
The following procedure is conducted under standard laboratory conditions
at 23.degree. C. (73.degree. F.) and 50% relative humidity. Using a 6
cm.times.23 cm cutting die, the tea bag material is cut, folded in half
lengthwise and sealed along two sides with a T-bar sealer to produce a 6
cm.times.6 cm tea bag square. The tea bag material utilized is a grade
1234 heat sealable material, obtainable from C. H. Dexter, Division of the
Dexter Corp.,Windsor Locks) Connecticut, U. S. A., or equivalent. Lower
porosity tea bag material should be used if required to retain fine
particles or fibers of polymeric gelling agent. 0.200 grams plus or minus
0.005 grams of the polymeric gelling agent is weighed onto a weighing
paper and transferred into the tea bag and the top (open end) of the tea
bag is sealed. An empty tea bag is sealed at the top and is used as a
blank. Approximately 300 milliliters of deionized water are poured into a
1,000 milliliter beaker. The blank tea bag is submerged in the deionized
water. The tea bag containing the polymeric 5 gelling agent (the sample
tea bag) is held horizontally to distribute the material evenly throughout
the tea bag. The tea bag is laid on the surface of the deionized water.
The tea bag is allowed to wet, for a period of no more than one minute,
and then is fully submerged and soaked for 60 minutes. Approximately 2
minutes after the first sample is submerged, a second set of tea bags,
prepared identically to the first set of blank and sample tea bags, is
submerged and soaked for 60 minutes in the same manner as the first set.
After the prescribed soak time has elapsed, for each set of tea bag
samples, the tea bags are promptly removed (using tongs) from the
deionized water. The samples are then centrifuged as described below. The
centrifuge used is a Delux Dynac II Centrifuge, Fisher Model No.
05-100-26, obtainable from the Fisher Scientific Co. of Pittsburgh, Pa.,
or equivalent. The centrifuge should be equipped with a direct read
tachometer and an electric brake. The centrifuge is further equipped with
a cylindrical insert basket having an approximately 2.5 inch (6.35 cm)
high outer wall with an 8.435 inch (21.425 cm) outer diameter, a 7.935
inch (20.155 cm) inside diameter, and 9 rows each of approximately 106
3/32 inch (0-238 cm) diameter circular holes equally spaced around the
circumference of the outer wall, and having a basket floor with six 1/4
inch (0.635 cm) diameter circular drainage holes equally spaced around the
circumference of the basket floor at a distance of 1/2 inch (1.27 cm) from
the interior surface of the outer wall to the center of the drainage
holes, or an equivalent. The basket is mounted in the centrifuge so as to
rotate, as well as brake, in unison with the centrifuge. The-sample tea
bags are positioned in the centrifuge basket with a folded end of the tea
bag in the direction of the centrifuge spin to absorb the initial force.
The blank tea bags are placed to either side of the corresponding sample
tea bags. The sample tea bag of the second set must be placed opposite the
sample tea bag of the first set; and the blank tea bag of the second set
opposite the blank tea bag of the first set, to balance the centrifuge.
The centrifuge is started and allowed to ramp up quickly to a stable speed
of 1,500 rpm, a timer is set for 3 minutes. After 3 minutes, the
centrifuge is turned off and the brake is applied. The first sample tea
bag and the first blank tea bag are removed and weighed separately. The
procedure is repeated for the second sample tea bag and the second blank
tea bag.
The Absorptive Capacity (AC) for each of the samples is calculated as
follows: AC =(sample tea bag weight after centrifuge minus blank tea bag
weight after centrifuge minus polymeric gelling agent weight) / (dry
polymeric gelling agent). The Absorptive Capacity value for use herein is
the average absorptive capacity of the two samples.
b. Extractable Polymer Content Determination
Depending upon the type of hydrogel-forming crosslinked polymeric gelling
agent involved, two different methods are used herein to calculate
extractable polymer content. For carboxylic acid-based polymeric gelling
agent a potentiometric procedure is used to determine extractables. For
sulfonic acid-based polymeric gelling agent, a gravimetric procedure is
employed. It should be noted that both of these procedures may provide
results that include in the total amount of extractable material those
extractable components in the polymeric gelling agent which are not
polymeric. Therefore, if a given polymer sample is known or believed to
contain significant amounts of non-polymeric extractable material, such
non-polymeric extractable material should be removed from the analyte in
conventional fashion before running the extractable polymer content
determination hereinafter described.
(1) Carboxylic Acid-Based Polymeric Gelling Agent
Extractable polymer content of carboxylic acid-based polymeric gelling
agent is determined by admixing the polymeric gelling agent with deionized
water for a period of time sufficient to substantially approach
equilibrium with respect to extraction of polymer material from the
hydrogel which is formed. The hydrogel/deionized water mixture is allowed
to settle and a portion thereof is filtered. An aliquot of this filtrate
is then taken, and the free acid groups on the polymer material dissolved
in this filtrate are titrated to pH 10 with base. All of the carboxylate
groups are then titrated to pH 2.7 with acid. These titration data are
then used to calculate the amount of extractable polymer in the polymeric
gelling agent sample.
(a) Preparation of the Extractable Polymer-Containing Filtrate Samples
1.0.40 to 0.41 g of polymeric gelling agent is accurately (to .+-.0.1 mg)
weighed into a 150 ml disposable beaker. If glass beakers are used they
must be acid washed prior to use. (Glassware should be washed three times
with dilute HCI [conc. HCI diluted 1:4 with dieionized water], then three
times with deionized water. This procedure removes trace of detergents and
other contaminants which would otherwise interfere with the titration.)
2. 75 ml of deionized water are added.
3. Samples are slowly stirred for a period of time sufficient to reach
equilibrium. Equilibrium is generally reached within 16 hour periods. If
extractable polymer content is to be measured as a function of time, then
1, 6, and 16 hour periods are generally sufficient to define the
extractables versus time curve.
4. Samples are allowed to settle for 15 minutes.
5. Using a 3 ml disposable syringe and 0.22 micron filters, enough solution
is filtered so that a 20 ml aliquot can be taken.
(b) Titration Conditions
1. If the titrations are to be performed manually, great care must be taken
to assure that equilibrium is reached after each addition of titrant.
2. A 20 ml aliquot of the filtrate is transferred to a 50 ml disposable
beaker. If glass beakers are being used, they must be acid washed prior to
use as noted herein before.
3. The aliquot is titrated to pH 10 with 0. 1N NaOH.
4. The aliquot is then back titrated to pH 2.7 with 0. 1N HCI.
5. Step 3 and 4 are performed on 20 ml of deionized water to obtain
titration blinks for both steps of the titration.
(c) Calculations
1. The amount of polymerized acid moleties (e.g., acrylic acid) (in
millimoles) in the supernatant aliquot (M.sub.a) is given by:
M.sub.a =(V.sub.a -V.sub.ab).times.N.sub.a millimoles (mm)
where:
V.sub.a = The volume (in ml) of acid required to titrate the aliquot to pH
10.;
V.sub.b = The volume (in ml) of acid required to titrate 20 mi of deionized
water to pH 10; and
N.sub.a = The normality (in meq/ml) of the acid (nominally 0.10 meq/ml)
2. The total amount of polymerized acid moleties (e.g. acrylic acid) plus
polymerized neutralized acid moleties (e.g., sodium acrylate) (in mm) in
the supernatant aliquot (M.sub.t) is given by:
M.sub.t =(V.sub.b -V.sub.bb)xNb millimoles
where:
V.sub.b = The volume (in ml) of base required to titrate the aliquot from
pH 10 down to pH 2.7;
V.sub.bb = The volume (in ml) of base required to titrate 20 ml of
deionized water from pH 10 down to pH 2.7; and
N.sub.b = The normality (in meq/mi) of the base (nominally 0.10 meq/ml).
3. The amount of polymerized neutralized acid moleties (e.g., sodium
acrylate) (in mm) in the original supernatant aliquot (M.sub.b) is given
by:
M.sub.b =M.sub.t -M.sub.a
4. The total amounts of polymerized acid moleties (W.sub.a) and polymerized
neutralized acid moieties(W.sub.b) (e.g., acrylic acid plus sodium
acrylate) extracted (in mg) are given by:
W.sub.a =M.sub.a xE.sub.a xD
and
W.sub.b =M.sub.b xE.sub.bx D
where:
E.sub.a = The equivalent weight of add moiety in polyacid moiety (e.g.,
acrylic acid in polyacrylic acid =72 meq/mg).
E.sub.b = The equivalent weight of neutralized acid moiety in neutralized
polyacid moiety (e.g., sodium acrylate in sodium polyacrylate =94 meq/mg).
D = The dilution factor (75 ml/20 ml=3.75).
5. The percent extractable polymer in the polymeric gelling agent sample
(e) is given by:
e=((W.sub.a +W.sub.b).times.100)/W
where: W=The sample weight in mg.
2. Sulfonic Acid-Containing Polvmeric Gelling Agent
Extractable polymer content of sulfonic acid-based polymeric gelling agent
is determined by a gravimetric procedure wherein hydrogel samples are
swollen overnight in deionized water, and the polymer content in the
nitrate is gravimetrically determined. The particular procedure of the
gravimetric extractables determination are set forth as follows:
Into a 500 ml Erlenmeyer flask is weighed accurately (to +/-0.1 mg) about
0.25 grams of dry polymeric gelling agent (W.sub.p). 250 ml of deionized
water is added and the mixture is stirred slowly for 1 hour. After this
hour has passed, stirring is stopped, and the swollen gel is allowed to
settle for about 16 hours. The supernatant is filtered using a 3 ml
disposable syringe and 0.22 micron filter to obtain at least 40 ml of
filtrate. Exactly 40 ml of filtrate is placed into a clean 100 ml
round-bottomed flask, and the solution is concentrated on a rotary
evaporator (water aspirator vacuum, bath temperature 55.degree. C.). The
remaining 2-3 ml of solution is transferred quantitatively to a tared
weighing vial with the aid of additional deionized water. The solution in
the weighing vial is reduced to dryness in an oven at 120.degree. C. The
vial is cooled, reweighed, and the weight of residue (W.sub.r) is
determined using the tare weight of the vial. The percent extractable
polymer (e) is calculated from the weight of dry polymer (W.sub.p) and
weight of residue (W.sub.r) by the following equation:
e=(W.sub.r .times.250.times.100)/(W.sub.p .times.40)
EXAMPLES
The following examples further describe and demonstrate embodiments within
the scope of the present invention. These examples are solely for the
purpose of illustration and are not to be construed as limitations of the
present invention as many variations are possible without departing from
the spirit or scope thereof.
______________________________________
Ingredient Example #
(wt. %) 1 2 3 4 5
______________________________________
Triclosan 0.30 0.30 0.08 0.08 0.08
Dipropylene Glycol
29.263 25.133 16.683
28.9083
28.629
Water 25.00 22.50 22.50 22.50 35.0
PEG-4.sup.1 -- -- 15.00 20.00 20.00
PEG-6.sup.2 30.00 -- -- -- --
PEG-8.sup.3 -- 25.00 -- -- --
Glycerol 8.00 -- 35.00 17.00 --
2-Hydroxypropyl-
-- 15.00 -- -- 9.00
glyceryl Ether.sup.4
Polyglycerol -- -- -- -- --
Sodium Stearate
5.60 5.50 5.50 5.30 5.25
Sodium Hydroxide
0.06 0.060 0.060 0.060 0.040
Solution
(50% solution)
PPG-3 myristyl ether
1.75 1.75 1.750 1.750 1.00
Color Solution
0.002 0.002 0.002 0.0017
0.001
Tetrasodium EDTA
0.025 0.025 0.025 0.025 0.025
Fragrance 5.20 5.00 3.40 4.40 1.00
______________________________________
.sup.1 Carbomer PEG200 .TM. Union Carbide Corporation (Danbury, CT, USA)
.sup.2 Carbomer PEG300 .TM. Union Carbide Corporation (Danbury, CT, USA)
.sup.3 Carbomer PEG400 .TM. Union Carbide Corporation (Danbury, CT, USA)
.sup.4 Prepared as described in U.S. Pat. No. 4,976,953 (Orr and
Sabatelli)
Ingredient Example #
(wt. %) 6 7 8 9
______________________________________
Triclosan 0.08 0.08 0.08 0.30
Dipropylene Glycol
-- 15.683 28.53 22.963
Water 22.00 22.50 22.50 10.00
PEG-4.sup.1 47.383 -- 25.00 8.00
PEG-6.sup.2 -- 30.00 -- --
PEG-8.sup.3 -- -- -- --
PEG-4 Stearate.sup.4
-- -- -- 25.00
Glycerol 18.00 -- -- 6.00
Propoxylated Glycerol
-- 20.00 -- --
Polyglycerol -- -- 12.00 15.00
Sodium Stearate
5.70 5.00 5.35 5.70
Sodium Hydroxide
0.06 0.060 0.060 0.060
Solution (50% solution)
PPG-3 myristyl ether
1.750 1.750 1.750 1.750
Color Solution
0.002 0.002 0.002 0.002
Tetrasodium EDTA
0.025 0.025 0.025 0.025
Fragrance 5.00 4.90 4.70 5.20
______________________________________
.sup.1 Carbomer PEG200 .TM. Union Carbide Corporation (Danbury, CT, USA).
.sup.2 Carbomer PEG300 .TM. Union Carbide Corporation (Danbury, CT, USA).
.sup.3 Carbomer PEG400 .TM. Union Carbide Corporation (Danbury, CT, USA).
.sup.4 Unipeg200 MS Universal PreservA-Chem. Inc. (Brooklyn, NY, USA).
The following procedure is followed to arrive at the compositions of
Examples 1-9. In a container equipped with stirring blace, add water,
along with polyhydroxy solvent(s) (PEG/Glycerol) and other polar solvents
(dipropylene glycol/polypropylene glycol-3 Mysristyl ether) as may be
applicable, deodorant active (Triclosan), and preservative (Tetrasodium
EDTA). Heat to about 79.degree.-85.degree. C. (175.degree.-185.degree.
F.), and stir at 50 rpm.
Add sodium stearate to the mixture and continue to stir. Once the solution
is clear, add sodium hydroxide. Cool the solution to 69.degree.-73.degree.
C. (157.degree.-163.degree. F.), add fragrance and mix thoroughly. Pack in
a conventional deodorant stick package at about 71.degree. C. (160.degree.
F.) and allow to cool to room temperature. The final product will be a
mild to the skin, efficacious, deodorant gel stick product.
______________________________________
Ingredient Example #
(wt. %) 10 11 12 13
______________________________________
Triclosan 0.300 0.080 0.080 0.300
Dipropylene Glycol
30.310 20.755 -- 43.905
Water 28.500 40.000 75.000
25.000
PEG-4.sup.1 14.299 20.599 12.903
0.599
PEG-8.sup.2 10.000 -- -- 17.205
Glycerol 8.105 10.00 5.000 10.00
Hydrogel-Forming
0.020.sup.3
0.100.sup.3
0.150.sup.3
0.0
Polymeric Gelling Agent
Sodium Stearate 5.000 5.000 5.300 4.500
Sodium Hydroxide
0.040 0.040 0.040 0.040
Solution (50% solution)
Color Solution 0.001 0.001 0.001 0.001
Tetrasodium EDTA
0.025 0.025 0.025 0.025
Fragrance 3.400 3.400 3.400 3.400
______________________________________
Ingredient Example #
(wt. %) 14 15 16
______________________________________
Triclosan 0.080 0.080 0.080
Dipropylene Glycol
13.695 -- --
Water 45.000 60.000 50.000
PEG-4.sup.1 20.599 20.599 21.049
Glycerol 11.560 10.400 20.000
Hydrogel-Forming
0.100.sup.4
0.250.sup.4
0.010.sup.3
Polymeric Gelling Agent
Sodium Stearate
4.700 5.200 5.300
Sodium Hydroxide
0.040 0.040 0.040
Solution (50% solution)
Color Solution 0.001 0.001 0.001
Tetrasodium EDTA
0.025 0.025 0.025
Fragrance 3.400 3.400 3.400
______________________________________
.sup.1 Carbowax PEG200 .TM. Union Carbide Corporation (Danbury, CT, USA).
.sup.2 Carbowax PEG400 .TM. Union Carbide corporation (Danbury, CT, USA).
.sup.3 Fibrous maleic anhydride/isobutylene crosslinked hydrogelforming
polymeric gelling agent, Fibersorb SA 7200H, from Camelot Technologies,
Inc. (Leominster, MA, USA).
.sup.4 Particulate acrylic acid crosslinked hydrogelforming polymeric
gelling agent, Aqualic .TM. L74 from Nippon Shokubai, Japan.
Alternatively, add Nalco N1181 from Nalco Chemical Company (Naperville,
IL, USA) can be used.
Formulations in Examples 10 to 16 are made as follows. Seventy to eighty
percent of total required water for the formulation is added to a mixing
vessel equipped with a rotor stator homogenizer. The hydrogel forming
polymeric gelling agent is added, with mixing at 9500 revolutions per
minute (rpm), at rate of 3 grams/minute until a clear hydrogel is formed
(Premix A). Heat Premix A to 68.degree.-74.degree. C.
(155.degree.-165.degree. F.) with stirring. In a separate container
equipped with stirring blade, add the remaining water along with the
polyhydroxy solvents, including glycerol, POE and other polar solvents as
may be applicable, deodorant active (triclosan), and preservative
(tetrasodium EDTA). Heat to about 79.degree.-85.degree. C.
(175.degree.-185.degree. F.), and stir at 50 rpm (Premix B). Add sodium
stearate to Premix B and mix until the solution is clear. Combine Premixes
A and B, cool the mixture to 69.degree.-73.degree. C. (157-163.degree.
F.). Add sodium hydroxide solution, fragrance and color solution, and mix
thoroughly. Pack in a conventional deodorant stick package at about
71.degree. C. (160.degree. F.) and allow to cool to room temperature. The
final product will be mild to the skin, efficacious, deodorant gel stick
product.
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